EP3177379B1 - Colonne et procédé de traitement thermique d'un fluide comprenant un conduit de retour - Google Patents

Colonne et procédé de traitement thermique d'un fluide comprenant un conduit de retour Download PDF

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Publication number
EP3177379B1
EP3177379B1 EP15747794.4A EP15747794A EP3177379B1 EP 3177379 B1 EP3177379 B1 EP 3177379B1 EP 15747794 A EP15747794 A EP 15747794A EP 3177379 B1 EP3177379 B1 EP 3177379B1
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Prior art keywords
column
mass transfer
liquid
transfer tray
flow
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EP15747794.4A
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German (de)
English (en)
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EP3177379A1 (fr
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Ulrich Hammon
Thomas Walter
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BASF SE
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BASF SE
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/0271—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of H2/CO mixtures, i.e. of synthesis gas
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/16—Fractionating columns in which vapour bubbles through liquid
    • B01D3/18—Fractionating columns in which vapour bubbles through liquid with horizontal bubble plates
    • B01D3/20—Bubble caps; Risers for vapour; Discharge pipes for liquid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/16—Fractionating columns in which vapour bubbles through liquid
    • B01D3/22—Fractionating columns in which vapour bubbles through liquid with horizontal sieve plates or grids; Construction of sieve plates or grids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/42—Regulation; Control
    • B01D3/4211—Regulation; Control of columns
    • B01D3/4261—Side stream
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78—Separation; Purification; Stabilisation; Use of additives
    • C07C45/783—Separation; Purification; Stabilisation; Use of additives by gas-liquid treatment, e.g. by gas-liquid absorption
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78—Separation; Purification; Stabilisation; Use of additives
    • C07C45/80—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78—Separation; Purification; Stabilisation; Use of additives
    • C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
    • C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C07C67/48—Separation; Purification; Stabilisation; Use of additives
    • C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation

Definitions

  • the present invention relates to a column for the thermal treatment of a fluid.
  • the column has a cylindrical, vertically oriented column body which forms a column cavity, and a mass transfer tray arranged in the column cavity, which forms a collecting surface.
  • the column is in particular a separation column.
  • the invention relates to a thermal separation process between at least one gas rising in a column and at least one liquid descending in the column.
  • thermal separation process examples of and thus element of the term "thermal separation process" used in this document are the fractionating condensation (cf., for example, US Pat DE 19924532 A1 . DE 10243625 A1 and WO 2008/090190 A1 and the rectification (in both, ascending vapor phase is conducted in countercurrent to descending liquid phase, the separation effect being due to the vapor composition being different in equilibrium from the liquid composition), the absorption (at least one ascending gas is countercurrently fed to at least one descending liquid the separation effect is due to the different solubility of the gas constituents in the liquid) and the desorption (the reversal process for absorption; the gas dissolved in the liquid phase is separated by partial pressure reduction; the partial pressure reduction of the liquid phase solutes at least partially by passing a carrier gas through the liquid phase is passed, this thermal separation process is also referred to as stripping; alternatively or additionally (at the same time as a combination), the partial pressure reduction can be effected by lowering the working pressure).
  • the separation of (meth) acrylic acid or (meth) acrolein from the product gas mixture of the catalytic gas phase oxidation can be carried out so that the (meth) acrylic acid or the (meth) acrolein by absorption into a solvent (eg water or an organic solvent ) or by fractional condensation of the product gas mixture first grundabgetrennt and that thereby resulting absorbate or condensate is subsequently further separated to obtain more or less pure (meth) acrylic acid or (meth) acrolein (cf., for example DE-10332758 A1 . DE 10243625 A1 . WO 2008/090190 A1 . DE 10336386 A1 . DE 19924532 A1 .
  • a solvent eg water or an organic solvent
  • acrylic monomers is used in this document to shorten “acrolein, acrylic acid and / or esters of acrylic acid”.
  • methacrylic monomers is used in this document to shorten “methacrolein, methacrylic acid and / or esters of methacrylic acid”.
  • the (meth) acrylic monomers contemplated herein are the following (meth) acrylic esters: hydroxyethylacrylate, hydroxyethylmethacrylate, hydroxypropylacrylate, hydroxypropylmethacrylate, glycidylacrylate, glycidylmethacrylate, methylacrylate, methylmethacrylate, n-butylacrylate, isobutylacrylate, isobutylmethacrylate, n-butylmethacrylate, tert-butyl acrylate, tert-butyl methacrylate, ethyl acrylate, ethyl methacrylate, 2-ethylhexyl acrylate, 2-ethylhexyl methacrylate, N, N-dimethylaminoethyl acrylate and N, N-dimethylaminoethyl methacrylate.
  • (Meth) acrylic monomers are important starting compounds for the preparation of polymers, e.g. be used as adhesives or as water super absorbent materials in hygiene articles use.
  • (meth) acrolein and (meth) acrylic acid are predominantly produced by catalytic gas phase oxidation of suitable C 3 - / C 4 precursor compounds (or precursor compounds thereof).
  • suitable C 3 - / C 4 precursor compounds or precursor compounds thereof.
  • propene and propane are preferably used as such precursor compounds.
  • methacrylic acid and methacrolein iso-butene and iso-butane are the preferred precursor compounds.
  • suitable starting materials are other compounds containing 3 or 4 carbon atoms, for example isobutanol, n-propanol or precursor compounds thereof, for example the methyl ether of isobutanol.
  • Acrylic acid can also be obtained by gas-phase catalytic oxidation of Acrolein be produced.
  • Methacrylic acid can also be produced by gas-phase catalytic oxidation of methacrolein.
  • product gas mixtures are normally obtained, from which the (meth) acrylic acid or the (meth) acrolein must be separated off.
  • Esters of (meth) acrylic acid are e.g. by direct reaction of (meth) acrylic acid and / or (meth) acrolein with the corresponding alcohols. However, in this case as well, first product mixtures are obtained from which the (meth) acrylic acid esters have to be separated off.
  • the separation columns in which these separation processes are carried out contain separating internals. These pursue in the thermal separation process the purpose of increasing the surface area for the separation in the separation column causing heat and mass transfer ("the exchange surface").
  • the separation columns used are those which contain at least one sequence of mass transfer trays, at least as part of the separating internals.
  • Mass transfer trays pursue the purpose of providing areas in the separation column in the form of liquid layers which form on them, with substantially closed liquid phases. The surface of the rising in the liquid layer and thereby distributing in the liquid phase vapor or gas flow is then the relevant exchange surface.
  • a succession of mass transfer trays is understood to mean a succession (one after the other) of at least two superimposed in the separation column, generally identically constructed (i.e., identical), mass transfer trays.
  • the clear distance between two mass transfer trays directly following one another in such a series (series) of mass transfer trays is made uniform (i.e., the mass transfer trays are arranged equidistantly in the separating column).
  • the simplest embodiment of a mass transfer tray is the so-called Regensiebêt. This is a plate or plate segments joined together to form a plate for the ascending gas or vapor phase (the Terms "gaseous” and “vaporous” are used synonymously in this document) distributed over the plate and substantially planar passage openings, eg round holes and / or slots, has (cf., eg DE 10230219 A1 . EP 1279429 A1 . US-A 3988213 and EP 1029573 A1 ). Exceeding openings (eg at least one downcomer (at least one drain segment)) do not have rain screen bottoms.
  • the cross section of the passages of a dual-flow tray is adapted in a conventional manner its load. If it is too small, the ascending gas flows through the passage openings at such a high speed that the liquid descending in the separation column is entrained substantially without separation effect. If the cross section of the passages is too large, ascending gas and descending liquid move past one another substantially without replacement, and the mass transfer tray runs the risk of running dry.
  • the separating effective working area of a Regensiebêts (dual-flow floor) has two limits.
  • a minimum limit speed of the rising gas must be given so that a certain liquid layer is held on the Regensiebêt to allow a segregation work of Regensiebêts.
  • the upper limit of the velocity of the rising gas is determined by the flood point, when the gas velocity leads to congestion of the liquid on the Regensiebêt and their rain is prevented.
  • the longest extent of the passage openings of a technical dual-flow tray is typically 10 to 80 mm (cf., for example DE 10156988 A1 ).
  • the passages within a rain screen are identical (ie, they all have the same geometric shape and cross section (cross sectional area)). In terms of application, its cross-sectional areas are circles. That is, preferred passages of Regensiebböden are circular holes.
  • the relative arrangement of the passage openings of a Regensiebteils advantageously follows a strict triangular division (cf., eg DE 10230219 A1 ). Of course, the passage openings within one and the same Regensiebêts can also be designed differently (vary over the Regensiebêt).
  • a sequence of rain sieve bottoms in a separation column comprises identical (identical) rain sieve trays, which are preferably arranged equidistantly one above the other.
  • the cross-section (preferably circular) within a dual-flow tray Although designed uniform, but within the sequence varies (eg decreases from bottom to top).
  • each dual-flow bottom of a corresponding bottom sequence concludes flush with the wall of the separation column.
  • a Regensiebêt usually has at most still openings, which serve the attachment of the soil Auflageringen or the like (see, eg DE 10159823 A1 ).
  • the liquid descending in the separation column drops into drops from dual flow soil to dual flow soil, i.e., the gas phase rising between the dual flow trays is traversed by a split liquid phase.
  • the falling on the respective bottom Regensiebêt drops are partially sprayed on impact.
  • the gas stream flowing through the passage openings bubbles through the liquid layer formed on the surface of the floor, whereby an intensive mass and heat exchange takes place between the liquid and the gas.
  • the cross section of a separation column is usually circular. This applies in a corresponding manner to the associated mass transfer trays.
  • sequences of mass transfer trays are distinguished with such liquid forced feed.
  • mass transfer trays are characterized in that they additionally have at least one downcomer in addition to the passage openings already described.
  • This is at least one drainage opening located in the mass transfer tray, which retains the liquid (eg, a drain weir (this may in the simplest embodiment extend the drain opening with a throat (a chimney, in the case of a circular drain opening of a tube) above)), and which drains into a passage tapering to the mass transfer tray below, which is generally center-symmetrical to an axis pointing in the column longitudinal direction.
  • the cross-section of the well may vary along this axis (e.g., taper) or be constant.
  • the liquid descending from a higher mass transfer tray can, within a sequence of such mass transfer trays, continue as an at least one feed of liquid to the next lower mass transfer tray of the sequence, regardless of the gas or vapor still rising through the passages of that mass transfer tray dismount.
  • Such a hydraulic lock can e.g. can be achieved by pulling the downcomer downwards (so far downwards) that it dives deep enough into the liquid layer located on the next lower mass transfer tray of the sequence (such a closure is also referred to in this document as " static closure ").
  • the liquid level required for this purpose can be determined on the lower mass transfer tray, e.g. be ensured by the height of appropriate drainage weirs.
  • such an embodiment has the disadvantage that the region of the lower mass transfer tray, which is located directly below the outlet cross section of a downcomer of the overlying mass transfer tray (the so-called inflow surface), can not have any passage openings for the rising gas and so not for the substance and heat exchange is provided between the liquid layer formed on the lower mass transfer tray and the rising gas.
  • the lower outlet end of the downcomer is raised so far that it no longer dips into the liquid layer located on the underlying mass transfer tray.
  • a sufficiently large gap in which form a bubble layer and a mass and heat exchange between a (on the lower mass transfer tray) accumulating liquid layer and a gas (rising through this floor) can take place.
  • the "inflow area" of the at least one downcomer on the mass transfer tray below may also have through openings, thus increasing the available exchange area of the mass transfer tray, and thus its separating effect.
  • a static fluid closure of the downcomer can be effected in this case, for example, by means of a mounted below the outlet end of the downcomer collecting cup.
  • the jacket wall of the collecting cup is pulled up so far that the outlet end of the downcomer dips into the collecting cup (it is also possible to allow the bottom edge of the downcomer to end at the upper edge of the collecting cup).
  • a raised drainage shaft can also be closed dynamically.
  • the downcomer can be closed, for example at its lower end with a bottom which is provided with outlet openings which are dimensioned so that the liquid dammed in the downcomer and the penetration of gas is prevented (see, eg EP 0882481 A1 and DE 10257915 A1 ).
  • the shaft closure is produced dynamically by the pressure loss that arises at the outlet openings.
  • the closure of the drainage shaft is characterized in that its outlet end immersed in jammed liquid, and dynamic closure effect constructive features at the outlet end of the downcomer that the exiting (leaking) liquid suffers a pressure loss in the downcomer backlog in selbigem descending liquid causes, which causes the closure.
  • a pressure loss can be caused by the fact that one selects the cross section of the outlet opening of the downcomer small compared to the average cross section of the shaft.
  • the execution of the at least one downcomer is relevant.
  • the cross-section of the at least one downcomer must be sufficiently large (usually the corresponding cross-sectional area is greater than the cross-sectional area of a passage opening), so that the liquid can safely descend through the at least one downcomer even at the maximum load of the separation column does not back up to the overlying ground.
  • it must be ensured that the hydraulic closure of the at least one downcomer still exists even with minimal liquid load.
  • a favorable flow rate of the liquid accumulated in the downcomer out of the downcomer in the process according to the invention is, for example, 1.2 m / s.
  • Such a liquid guide on a mass transfer tray within a sequence of identical mass transfer trays shall be referred to herein as a cross flow, the sequence of such identical mass transfer trays as a succession of identical cross flow mass transfer trays and the single mass transfer tray within the sequence as cross flow mass transfer trays.
  • the cross-flow mass transfer tray is a cross-flow sieve tray.
  • the at least one downcomer Apart from the at least one downcomer, it has passage openings for the gas rising in a separating column, for the design of which basically all the embodiments mentioned in the rain screen floor come into consideration.
  • a cross-flow sieve bottom as through-openings also has circular bores which, in terms of application technology, advantageously also have a uniform radius.
  • the at least one downcomer makes it possible for the liquid descending in a separation column to pass through a succession of crossflow trays independently of the flow path of the successive rising vapor (through the passage openings) from a higher crossflow sieve tray to the next descend lower-lying cross-flow sieve tray can.
  • the liquid flows in cross-flow from the at least one inlet of the lower floor formed by the at least one outlet of the higher cross-sieve tray to the at least one downcomer (to the at least one drain) of the lower floor, e.g. the height of at least one drain weir, via which the liquid can flow to the at least one downcomer, ensures the desired liquid level on the lower cross-flow sieve bottom.
  • the liquid is held by the back pressure of the rising in the separation column steam on the cross-flow sieve tray.
  • the liquid may rain through the passage openings, which reduces the separating effect of the cross-flow sieve tray and / or leads to dry running of the cross-flow sieve tray.
  • steam diverter hoods (bells, upturned cups) are usually attached (in the simplest case these can be bolted to the neck (e.g., front and back) and are practically slipped over the neck) which dip into the liquid accumulated on the floor.
  • the rising through the respective passage opening steam first flows through the neck into the associated hood, in which it is diverted to then, in contrast to the cross-flow sieve bottom, parallel to the bottom surface of the hood in the self-accumulated liquid to flow (such "Parallel outflow" in the process according to the invention is generally advantageous insofar as it can "blow off” polymer particles formed in an undesired manner and thereby cause a self-cleaning effect).
  • the gas streams (vapor streams) emerging from neighboring hoods which are preferably distributed equidistantly over the trays, swirl the liquid accumulated on the bottom and form a bubbling layer in the same, in which the material and heat exchange takes place.
  • Such cross-flow mass transfer trays are also referred to as cross-flow bubble trays or cross-flow tray trays. Since they also contain liquid accumulated with low rising gas (vapor) and thus run the risk of running dry, they are also referred to as hydraulically sealed cross flow trays. In comparison to cross-flow sieve trays, they usually require higher investment costs and cause higher pressure losses of the gas rising through them. In contrast to the simple sieve passage opening of a sieve tray, the passage opening of these trays, which is designed as described, is also referred to as bell passage opening or hood passage opening.
  • the bell edge can have very different shapes in cross-flow bubble trays (see. DE 10243625 A1 and Chemie-Ing. Techn. 45th 1967 / Nr. 9 + 10, pp. 617-620 ).
  • Figure 3 out Chemie-Ing. Techn. 45 years. 1973 / No. 9 + 10, p. 618 shows some examples of the serrated and slotted edge.
  • the serrations and slots are usually shaped so that the steam entering the mass stored on the mass transfer tray out of the bell dissolves as easily as possible into a large number of bubbles or jets of steam.
  • FIG. 3 shows exemplary embodiments of bell rims having a sawtooth-like structure, the teeth of which are additionally provided with vanes (baffles) ("raised slots").
  • the guide vanes are to impose a tangential exit direction on the gas stream (vapor stream) emerging from the bent sawtooth-like slots (direct the gas exit into the liquid in an oblique direction), whereby the surrounding liquid receives a directed impulse of movement, which interacts with the arrangement of the bells (steam deflection hoods). can result in a directional liquid flow on the cross-flow bubble tray overlaying the cross-flow established across the mass transfer tray (often such upturned slots are also referred to as drive slots).
  • the liquid does not flow on a lower cross-flow Thormann bottom directly across the ground, but driven in a manner described above, meandering from the at least one inlet to the at least one drain.
  • the space between two cross-flow directionally arranged hoods of a cross-flow Thormannteils each forms a groove in which the liquid flows.
  • the details of a cross-flow Thormannteils also usually carried out so that the liquid flows in two in the cross-flow direction each successive grooves in countercurrent (see, eg. FIG. 3 the DE 10243625 A1 ).
  • the resulting meandering of the cross-flow extends the flow path of the liquid from the at least one inlet to the at least one drain, which favors the separation effect of a cross-flow Thormannteils.
  • cross-flow mass transfer tray As a valve (as a valve passage opening).
  • the resulting cross-flow mass transfer trays are referred to as cross-flow valve trays (cf., for example, US Pat. DD 279822 A1 . DD 216633 A1 and DE 102010001228 A1 ).
  • cross-flow valve floors subsumes in this document thus cross-flow mass transfer trays, the passage openings (bottom holes) with stroke-limited plate, ballast or lifting valves (floating flaps) that adjust the size of the steam passage opening of the respective column load.
  • the passage openings of the bottom for the aforementioned purpose with upwardly movable lids or plates (discs) are covered.
  • the lids (plates, disks) are raised by the gas flow in an additionally via the respective passage opening mounted (which is usually firmly anchored to the ground) corresponding guide frame (guide cage) and finally reach a gas load corresponding lifting height (instead of Guide cage, the disc can also have anchored with the floor upwardly movable valve legs whose upward mobility is limited upwards).
  • the ascending through the passage opening gas flow is deflected at the bottom of the raised lid (plate, disc) in a similar manner as in the bell (at a bell passage opening) and emerges from the under the raised plate (lid, disc) resulting emergence area and as in the Bubble tray parallel to the bottom into the liquid stored on it.
  • the plate stroke thus controls the size of the gas outlet area and adapts itself to the column load until the upper end of the guide cage limits the maximum possible lifting height.
  • the plates may have downwardly directed spacers, so that at low gas load, the valve closes only so far that created by the spacers space still allows intensive mixing of the horizontal gas outflow with the cross-flow liquid. Spacers also counteract adhesion of the valve disc on the ground.
  • valve elements of a cross-flow valve bottom By suitable design of the valve elements of a cross-flow valve bottom, the Adjusted blowing direction of the valve element and thus the liquid forced operation on the cross-flow valve bottom are additionally influenced (see, for. DD 216 633 A1 ).
  • the principle of cross-flow valve trays and usable for the purposes of the present document valve bottoms is found, for. In Technical Progress Reports, Volume 61, Fundamentals of Column Sizing, pages 96 to 138 executed.
  • fixed valves In addition to the above-described movable valves, the expert also knows fixed valves. These are usually disc-shaped, or trapezoidal, or rectangular units that are punched out of the bottom plate and connected to it via upstanding fixed legs.
  • the bell size can be changed in cross-flow bubble trays or by using z. B. plates (lids) with different weight at cross-flow valve floors can be compensated in this regard, so that the mass transfer floor over its cross-section substantially uniform guest (where the liquid level is smaller on the cross-flow mass transfer tray, the seat height of the bell is appropriate in terms of application
  • the seat height of the bell can also be set deeper, for example, by shortening the length of the corresponding chimney, at the end of which the bell may be screwed, in a targeted manner, or alternatively, by shortening the weight of the lifting plate (lifting lid) or additionally, for example, the prong / slot structure of the bellhousing may also be varied to provide the desired flow resistance compensation, ideally, adjustment via the crossflow mass transfer tray is such that, during operation of the separation column, each of those on a crossflow bell bottom n bell located causes the same flow resistance for the rising gas).
  • the cross-sectional area usually more than 200 times smaller than the total cross-sectional area of all other openings of the Querstromstoff head convinceds (not including the cross section of the at least one downcomer), do not form (effective) through-openings the rising through the cross-flow mass transfer tray gas and self selbigen therefore not be attributed.
  • openings may be tiny idle bores through which hydraulically sealed crossflow trays may run empty when a separation column is switched off. Also, such openings can serve Verschraubungs section.
  • the prior art recommends the use of sequences of at least two structurally identical (identically designed) cross-flow mass transfer trays including separating columns containing separation internals which are used to carry out thermal separation processes between at least one gas stream rising in the separation column and at least one liquid stream descending in the separation column and at least one of the streams contains at least one (meth) acrylic monomer.
  • the writings recommend DE 19924532 A1 .
  • Characteristic of the sequences of the cross-flow mass transfer trays recommended in the prior art is that the lower of two consecutive crossflow mass transfer trays in the direction of the cross flow from its at least one inlet to its at least one downcomer only in the region between the at least one inlet and the at least one downcomer (the at least one drainage opening) has passage openings (cf., for example, FIGS Figures 3 and 4 the DE 10243625 A1 , the FIG. 1 the DD 279822 A1 , the FIG. 1 the DD 216633 A1 and the illustration 1 out Chemie-Ing.-Techn. Volume 45, 1973 / No. 9 + 10, pages 617 to 620 ).
  • the CA 2017980 A1 describes a distillation reactor in which a catalyst is replaced by a fresh or regenerated catalyst.
  • the liquid catalyst which has collected on a collecting tray, removed via an outlet.
  • the withdrawn catalyst is fed to a separator in which solid components of the catalyst are separated.
  • the liquid catalyst is pumped back to the distillation reactor.
  • a return opening is provided, which is arranged below the removal of the catalyst.
  • DE 19924532 A1 a process of fractionally condensing an acrylic acid-containing product gas mixture of a heterogeneously catalyzed gas-phase partial oxidation of C3 precursors of acrylic acid with molecular oxygen.
  • the separation column used has both dual-flow trays and hydraulically sealed crossflow trays as separation-effective internals.
  • EP 00009545 a process for recovering acrylic acid from a gaseous reactor effluent containing acrylic acid, acrolein, water and impurities.
  • a problematic property of (meth) acrylic monomers is their tendency to undesired polymerization, which, especially in the liquid phase, can not be completely suppressed even by the addition of polymerization inhibitors.
  • a disadvantage of known separation columns is that, when the thermal separation process is carried out continuously over a longer period of operation, the mass transfer trays are comparatively frequently used to form unwanted polymer. This is particularly disadvantageous because the operator of the thermal separation process due to the unwanted Polymerisataise must interrupt the thermal separation process again and again to remove the polymer formed. The same can indeed partially or completely close the passages of the mass transfer tray.
  • radical polymerization of (meth) acrylic monomers is usually highly exothermic, i. H. under strong heat. There is a risk that the polymerization proceeds so vigorously that the separation column containing the polymerization mixture explodes.
  • the invention relates to a column for the thermal treatment of a fluid having a cylindrical, vertically oriented column body, which forms a column cavity, and a mass transfer tray arranged in the column cavity, which forms a collecting surface.
  • the column according to the invention further comprises a circulation device having at least one drain opening formed in the column body above the collection surface, a circulation line in fluid communication with the drain opening and at least one return port fluidly connected to the circulation line and formed in the column body above the collection surface.
  • top refers to the orientation of the column during operation.
  • the undesired polymer is formed in particular in so-called dead zones of the mass transfer tray.
  • the residence time of the fluid in the mass transfer tray is particularly long.
  • Such a long residence time favors the polymerization.
  • circulation means a liquid circulation can be generated on the collecting surface of the mass transfer tray, which avoids the formation of dead zones.
  • the liquid stream takes with it any fluid residues.
  • the residence time of liquid on the collecting surface of the mass transfer tray is thereby reduced.
  • the residence time distribution becomes narrower, that is, there are fewer volumes of liquid remaining on the mass transfer tray for a longer time.
  • this can prevent the polymer from partially or completely closing through openings in the mass transfer tray.
  • the risk of explosion caused by the polymerization mixture is reduced.
  • the drain opening is arranged directly above the lowest area of the collecting surface of the mass transfer tray.
  • the lower edge of the discharge opening may be arranged at the same height as the deepest region of the collecting surface, so that the liquid located on the collecting surface is substantially completely to the discharge opening can run without residues remaining on the collecting surface.
  • this effectively prevents the formation of polymer when a fluid is treated in the column which tends to polymerize.
  • a plurality of vertically spaced mass transfer trays are arranged in the column cavity and the discharge opening and the return opening are arranged vertically between two adjacent vertically spaced mass transfer trays.
  • the ratio of the vertical distance of the deepest portion of the collecting surface of the mass transfer tray from the lower edge of the discharge port to the vertical distance of the deepest portion of the collecting surface of the mass transfer tray from the bottom of the overlying mass transfer tray is in a range of 0 to 0.3 , in particular in a range of 0 to 0.1.
  • the return opening can open in the column according to the invention either above the drain opening in the column cavity or the return opening opens at the same height as the drain opening in the column cavity.
  • the arrangement of the return opening is selected relative to the drain opening so that on the collecting surface of the mass transfer tray, a liquid circulation is generated, which reaches all areas of the mass transfer tray, so that in particular form no dead zones.
  • the ratio of the vertical distance of the deepest portion of the mass transfer tray collecting surface from the upper edge of the return aperture to the vertical distance of the lowest portion of the mass transfer tray collecting surface from the bottom of the immediately above the mass transfer tray is in a range of 0 to 0.3, in particular in a range of 0 to 0.2.
  • a nozzle for generating a liquid jet when the liquid enters the column cavity is arranged in the return opening. If several return openings are arranged in the column, in particular each of these return openings can have such a nozzle. By means of the nozzle or the nozzles can be prevented even more effectively that dead zones arise, in which polymer is formed in the treatment of a corresponding fluid.
  • the circulation line and the return opening or the return openings are in particular arranged so that the recirculated liquid enters radially into the column cavity.
  • this more effectively prevents the formation of dead zones.
  • a plurality of spaced apart return openings are formed in the column body. These return openings are each in fluid communication with the circulation line.
  • the liquid discharged via the drainage opening can in this way be recycled to the column cavity above the mass transfer tray at several points.
  • this makes it even more effective that no dead zones form at the collecting tray.
  • the mass transfer tray or at least one bottom of the column has passage openings for gas rising from below.
  • cylindrical bodies extend upwards. These cylindrical bodies are provided in particular at a certain distance with hoods, caps or roofs, so that gas can escape laterally from the cylindrical bodies, without the abraschende from the overlying mass transfer medium liquid can move in countercurrent to the gas.
  • These bodies also referred to as chimneys, which are perpendicular to the mass transfer tray, may in special cases have a square, rectangular, elliptical cross-sectional area in addition to a circular cross-section.
  • the distance (A) of the hoods, caps or roofs to the cylindrical body with diameter (D) is usually A ⁇ 2D.
  • This type of floor is a chimney floor, which collects at least part of the fluid dissipating from the upper floor in the space between the chimneys, where it can be fed from there to a purposeful other use.
  • the upper edges of the cylindrical body form overflow edges.
  • the ratio of the vertical distance of the lowest area of the collecting surface of the mass transfer tray from the lower edge of the discharge opening to the vertical distance of the lowest region of the collecting surface of the mass transfer tray from the height of the lowest overflow edge of the cylindrical body is z. B. in a range of 0 to 0.1, in particular in one Range from 0 to 0.05.
  • the ratio of the vertical distance of the deepest portion of the mass transfer tray collecting surface from the upper edge of the return port to the vertical distance of the deepest portion of the mass transfer tray collecting surface from the height of the lowermost overflow edge of the cylindrical bodies is in a range of 0 to 0 , 9, in particular in a range of 0 to 0.3.
  • the return openings are arranged relative to the cylindrical bodies so that a meandering liquid flow results on the collecting surface of the mass transfer tray.
  • the liquid flow can in particular reach all areas of the collection surface on the mass transfer tray so that no dead zones form on the collecting surface despite the interruptions by the cylindrical bodies.
  • the circulation line has a junction for supplying a further liquid.
  • an inert liquid or a liquid with polymerization inhibitors is supplied via this junction.
  • a pump is arranged in the circulation line with which liquid accumulating on the collecting surface of the mass transfer tray can be pumped off and this can be fed back to the column cavity through the return opening.
  • the liquid flow can be controlled or regulated on the mass transfer tray.
  • the pump or control valve may be further coupled to a sensor which measures the level of liquid on the collecting surface of the mass transfer tray. Depending on this liquid level, the pump can then regulate the circulation and / or the liquid removal of the liquid.
  • the column according to the invention can be used in particular as a separation column.
  • the separation column has a sequence of mass transfer trays.
  • mass transfer trays in particular the floors mentioned above are used, ie mass transfer trays without forced operation, such as rain screen floors and dual-flow trays, and mass transfer trays with a liquid forced operation, such.
  • the clear distance between two directly successive trays within the column according to the invention is in particular not more than 700 mm, preferably not more than 600 mm or not more than 500 mm.
  • the clear distance within the floor sequence is 300 to 500 mm.
  • the ground clearance should not be less than 250 mm.
  • the height of the column body is, for example, greater than 5 m, in particular greater than 10 m. However, it is also possible that the height of the column body exceeds 30 m or 40 m.
  • the invention further relates to a thermal separation process between at least one gas rising in a column as described above and at least one liquid descending in the column.
  • the liquid introduced via the return opening is introduced below the liquid level on the collecting surface.
  • the ascending gas and / or the descending liquid contains in particular (meth) acrylic monomers.
  • the thermal separation process according to the invention may e.g. a fractional condensation process for separating acrylic acid from a product gas mixture containing acrylic acid of a heterogeneously catalyzed gas phase partial oxidation of a C3 precursor compound (in particular propene and / or propane) of the acrylic acid with molecular oxygen to acrylic acid.
  • a C3 precursor compound in particular propene and / or propane
  • the separation column (condensation column) can, as in the publications DE 10243625 A1 or. WO 2008/090190 A1 be executed described, it is envisaged that at least partially the above-described circulation facilities are provided in the soils used there.
  • the tendency to polymerize is particularly great due to the use of (meth) acrylic monomers.
  • Such undesired polymerization is prevented in the process according to the invention in that the liquid collecting on the collecting surface of a mass transfer tray is pumped out through the discharge opening and is returned to the column cavity via the return opening or via the return openings.
  • the embodiment described below relates to a separation column 1, as z. B. in a process of fractional condensation for the separation of acrylic acid from an acrylic acid-containing product gas mixture of a heterogeneously catalyzed gas phase partial oxidation of a C3 precursor compound (in particular propene and / or propane) of acrylic acid is used with molecular oxygen to acrylic acid.
  • a C3 precursor compound in particular propene and / or propane
  • Fig. 1 is the known separation column 1 shown schematically. It comprises a cylindrical column body 2 whose axis is vertically aligned.
  • the column body 2 is essentially a hollow cylinder. That is, the shell of the column body 2 forms a column cavity 3.
  • the column body 2 is made of stainless steel.
  • the separation column 1 is normally thermally isolated in a conventional manner.
  • the height of the separation column 1 is 40 m.
  • mass transfer trays 4 are fixed, which are aligned horizontally and vertically spaced from each other.
  • the mass transfer trays 4 serve as separating internals which improve the material separation in the separation column 1.
  • FIG. 1 shown partial view of one of the mass transfer trays 4 is shown.
  • the mass transfer tray 4 in this case is a chimney tray.
  • This mass transfer tray 4 comprises a horizontally mounted in the column body 2 plate which forms the collecting surface 5 on the top.
  • In the plate passage openings 20 are formed.
  • chimneys 6 are used.
  • 20 fluid-tight cylindrical body 8, which are also referred to as a fireplace body, are inserted into the passage openings. Up to the upper edge 23 of the cylindrical body 8, liquid 21 can accumulate on the collecting surface 5.
  • the opening formed within the cylindrical body 8 is covered by a cover 7, that is, the opening is shielded against dripping liquid.
  • Such fireplace floors are known.
  • a circulation device 9 is now provided.
  • This circulation device 9 comprises a drain opening 10, which is formed directly above the collecting surface 5 in the shell of the column body 2.
  • a circulation line 11 connects. Through the drain opening 10 liquid 21, which accumulates on the collecting surface 5, led out of the column cavity 3.
  • a pump 12 is arranged, which promotes the liquid led out via the circulation line 11 to a return opening 14.
  • the return opening 14 is arranged above the upper edge of the cylindrical body 8 of the chimneys 6.
  • the circulation line 11 opens into this return opening 14, wherein in the return opening 14 and at the end of the circulation line 11, a nozzle 15 is arranged. Via the nozzle 15, the liquid is injected above the drain opening 10 back to the mass transfer tray 4.
  • the circulation line 11 and the return opening 14 are arranged so that the recirculated liquid radially into the Column cavity 3 enters.
  • the nozzle 15 is designed so that in all areas on the collecting surface 5 of the mass transfer tray 4, a liquid flow is generated, which prevents the result that long residence times of liquid volumes on the collecting surface.
  • the return opening 14 is arranged at the same height as the discharge opening 10 or at least below the upper edge 23 of the cylindrical body 8 of the chimneys 6.
  • the return opening 14 is arranged in this case, optionally below the liquid level 22 on the collecting surface 5.
  • a so-called propulsion jet nozzle 15 is arranged in the return opening 14, through which the liquid is injected into the standing liquid 21, whereby a liquid flow is generated on the collecting surface 5.
  • FIG. 2 The other facilities of the circulation device 9 are in FIG. 2 not shown for reasons of clarity. They are the same as they are already related to FIG. 1 have been described.
  • FIG. 3 For example, possible vertical arrangements of the collecting surface 5, the discharge opening 10, the return opening 14, the liquid level 22, the upper edges 23 of the cylindrical body 8 and the bottom 26 of the immediately above the mass transfer tray 4 are illustrated.
  • the collecting surface 5 is at the height L1
  • the lower edge 24 of the drain opening 10 is at the height L2
  • the upper edge 25 of the rear opening 14 is arranged at the height L3.
  • the liquid level 22 is arranged at the height L4.
  • the cylindrical body 8 of the chimneys 6 form at their upper edges 23 overflow edges.
  • the lowest overflow edge of the cylindrical body 8 is arranged at the height L5.
  • the underside 26 of the immediately above the collecting surface 5 arranged mass transfer tray 4 is arranged at the height L6.
  • the return opening 14 and the drain opening 10 are arranged between the two adjacent mass transfer trays 4 and below the liquid level 22. Further, the ratio of the vertical distance of the collecting surface 5 of the mass transfer tray 4 from the lower edge 24 of the discharge port 10 to the vertical distance of the collecting surface 5 of the mass transfer tray 4 from the height L5 of the lowermost overflow edge of the cylindrical body 8 in a range of 0 to 0 , 1, ie: 0 ⁇ Section L 1 - L 2 Section L 1 - L 5 ⁇ 0.1
  • the ratio of the vertical distance of the collecting surface 5 of the mass transfer tray 4 from the upper edge 25 of the return opening 14 to the vertical distance of the collecting surface 5 of the mass transfer tray 4 from the height L5 of the lowest overflow edge of the cylindrical body 8 is in a range from 0 to 0, 9, ie: 0 ⁇ Section L 1 - L 3 Section L 1 - L 5 ⁇ 0.9
  • the collecting tray 4 is not a chimney tray but a differently shaped collecting tray 4, which has no cylindrical body 8, the ratio of the vertical distance of the collecting surface 5 of the mass transfer tray 4 from the lower edge 24 of the discharge opening 10 to the vertical distance of the collecting surface 5 of the mass transfer tray 4 from the bottom 26 of the immediately above arranged mass transfer tray 4 in a range of 0 to 0.3, that is it applies: 0 ⁇ Section L 1 - L 2 Section L 1 - L 5 ⁇ 0.3
  • the ratio of the vertical distance of the collecting surface 5 of the mass transfer tray 4 from the upper edge 25 of the return port 14 to the vertical distance of the collecting surface 5 of the mass transfer tray 4 from the bottom 26 of the immediately above the mass transfer tray 4 in a range of 0 to 0.3 ie: 0 ⁇ Section L 1 - L 3 Section L 1 - L 5 ⁇ 0.3
  • a channel formed in the mass transfer tray 4 can open into the discharge opening 10.
  • the circulation line 11 can open into a plurality of return openings 14.
  • the circulation line 11 further includes a junction 13. At this junction 13 opens a supply line 16 for a further liquid in the circulation line 11 on.
  • the supply line 16 has a valve 17, via which the liquid supply can be controlled or regulated in the circulation line 11.
  • FIG. 4 is a cross section at the height of the return opening 14 of the column 1 according to the invention shown. It shows FIG. 4 a still further embodiment in which not only a return opening 14 is formed in the column body 2, but a plurality of return openings 14-1, 14-2 and 14-3. These return openings 14-1 to 14-3 are connected via a ring line 18 to the circulation line 11. The return openings 14-1 to 14-3 are arranged in this case relative to the chimneys 6 so that a meandering liquid flow 19 results on the collecting surface 5 of the mass transfer tray 4.
  • the return openings 14-1, 14-2 and 14-3 and the drain opening 10 can be as above with reference to FIG. 3 explained to be arranged in a vertical sense.
  • the process is a thermal separation process between at least one gas rising in the separation column 1 and at least one liquid descending in the separation column 1.
  • the ascending gas and / or the descending liquid contains (meth) acrylic monomers.
  • a fractional condensation is carried out to separate acrylic acid from a product gas mixture containing acrylic acid of a heterogeneously catalyzed gas phase partial oxidation of a C3 precursor compound (in particular propene and / or propane) of the acrylic acid with molecular oxygen to acrylic acid in a separating column 1 containing separating internals.
  • the separation column 1 contains from bottom to top several mass transfer trays 4. For example, initially dual-flow trays and then cross-flow hood floors or chimney trays are arranged, in which at least in part a respective circulation device 9 is formed, as described above. Otherwise the procedure is carried out as described in the scriptures DE 19924532 A1 . DE 10243625 A1 and WO 2008/090190 A1 is described. However, liquid is continuously pumped from the collecting surfaces 5 of the mass transfer trays 4 by means of the circulation means 9 and the collecting surfaces 5 at the respective mass transfer tray 4 fed back via the return opening 14 or the return openings 14-1 to 14-3.
  • C3 precursor of acrylic acid is taken to mean those chemical compounds which are obtainable formally by reduction of acrylic acid.
  • Known C3 precursors of acrylic acid are e.g. Propane, propene and acrolein. But also compounds such as glycerol, propionaldehyde, propionic acid or 3-hydroxypropionic acid are among these C3 precursors count.
  • the heterogeneously catalyzed gas phase partial oxidation with molecular oxygen is at least partially an oxidative dehydrogenation.
  • said C3 precursors of acrylic acid typically with inert gases such as e.g.
  • diluted molecular nitrogen, CO, CO2, inert hydrocarbons and / or steam passed in admixture with molecular oxygen at elevated temperatures and optionally elevated pressure over transition metal mixed oxide catalysts and oxidatively converted into an acrylic acid-containing product gas mixture.
  • the acrylic acid-containing product gas mixture of a heterogeneously catalyzed gas phase partial oxidation of C3 precursors (eg propene) of acrylic acid with molecular oxygen to solid state catalysts based on the total amount of (indicated in) specified constituents, the following contents : 1 to 30% by weight Acrylic acid, 0.05 to 10% by weight molecular oxygen, 1 to 30% by weight Water, 0 to 5% by weight Acetic acid, 0 to 3% by weight propionic acid, 0 to 1% by weight Maleic acid and / or maleic anhydride, 0 to 2% by weight acrolein, 0 to 1% by weight Formaldehyde, 0 to 1% by weight furfural, 0 to 0.5% by weight benzaldehyde, 0 to 1% by weight Propen, and as residual amount of inert gases such as nitrogen, carbon monoxide, carbon dioxide, methane and / or propane.
  • C3 precursors eg propene
  • inert gases such
  • the partial gas phase oxidation itself can be carried out as described in the prior art. Starting from propene, the partial gas phase oxidation for example, be carried out in two successive oxidation stages, as for example in the EP 700 714 A1 and in the EP 700 893 A1 are described. Of course, but also in the DE 19740253 A1 as well as in the DE 19740252 A1 cited gas phase partial oxidations are used.
  • the temperature of the product gas mixture leaving the partial gas phase oxidation is 150 to 350 ° C., frequently 200 to 300 ° C.
  • the hot product gas mixture is expediently first cooled to a temperature of 100 to 180 ° C, before it is conducted for the purpose of fractional condensation in the region C (the bottom) of the separation column 1.
  • the pressure prevailing in the separation column 1 operating pressure is usually 0.5 to 5 bar, often 0.5 to 3 bar and often 1 to 2 bar.

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Claims (15)

  1. Colonne (1) pour le traitement thermique d'un fluide, comprenant un corps de colonne cylindrique orienté verticalement (2), qui forme une cavité de colonne (3), et un plateau d'échange de matière (4) agencé dans la cavité de colonne (3), qui forme une surface de collecte (5), et
    un dispositif de circulation (9), comprenant au moins une ouverture d'évacuation (10) formée dans le corps de colonne (2) au-dessus de la surface de collecte (5), une conduite de circulation (11) en connexion fluidique avec l'ouverture d'évacuation (10), et au moins une ouverture de recyclage (14 ; 14-1 à 14-3) en connexion fluidique avec la conduite de circulation (11), formée dans le corps de colonne (2) au-dessus de la surface de collecte (5),
    caractérisée en ce que
    le plateau d'échange de matière (4) comprend des ouvertures de passage (20) pour un gaz ascendant depuis le bas, et des corps cylindriques (8) s'étendent vers le haut au niveau des ouvertures de passage (20),
    les bords supérieurs (23) du corps cylindrique (8) formant des bords de débordement, et le rapport entre l'écart vertical entre la zone la plus basse (L1) de la surface de collecte (5) du plateau d'échange de matière (4) et le bord supérieur (25) de l'ouverture de recyclage (14 ; 14-1 à 14-3) et l'écart vertical entre la zone la plus basse (L1) de la surface de collecte (5) du plateau d'échange de matière (4) et la hauteur (L5) du bord de débordement le plus inférieur du corps cylindrique (8) se situant dans une plage allant de 0 à 0,9, notamment dans une plage allant de 0 à 0,3.
  2. Colonne (1) selon la revendication 1, caractérisée en ce que le bord inférieur (24) de l'ouverture d'évacuation (10) est agencé directement au-dessus de la zone la plus basse de la surface de collecte (5) du plateau d'échange de matière (4).
  3. Colonne (1) selon la revendication 1 ou 2, caractérisée en ce que plusieurs plateaux d'échange de matière espacés verticalement (4) sont agencés dans la cavité de colonne (3), et l'ouverture d'évacuation (10) et l'ouverture de recyclage (14 ; 14-1 à 14-3) sont agencées verticalement entre deux plateaux d'échange de matière espacés verticalement voisins (4).
  4. Colonne (1) selon la revendication 3, caractérisée en ce que le rapport entre l'écart vertical entre la zone la plus basse (L1) de la surface de collecte (5) du plateau d'échange de matière (4) et le bord inférieur (24) de l'ouverture d'évacuation (10) et l'écart vertical entre la zone la plus basse (L1) de la surface de collecte (5) du plateau d'échange de matière (4) et le côté inférieur (26) du plateau d'échange de matière agencé directement au-dessus (4) se situe dans une plage allant de 0 à 0,3, notamment dans une plage allant de 0 à 0,1.
  5. Colonne (1) selon l'une quelconque des revendications précédentes, caractérisée en ce que l'ouverture de recyclage (14 ; 14-1 à 14-3) débouche au-dessus de l'ouverture d'évacuation (10) dans la cavité de colonne (3).
  6. Colonne (1) selon l'une quelconque des revendications 1 à 4, caractérisée en ce que l'ouverture de recyclage (14 ; 14-1 à 14-3) débouche à la même hauteur que l'ouverture d'évacuation (10) dans la cavité de colonne (3).
  7. Colonne (1) selon l'une quelconque des revendications 3 ou 6, caractérisée en ce que le rapport entre l'écart vertical entre la zone la plus basse (L1) de la surface de collecte (5) du plateau d'échange de matière (4) et le bord supérieur (25) de l'ouverture de recyclage (14 ; 14-1 à 14-3) et l'écart vertical entre la zone la plus basse (L1) de la surface de collecte (5) du plateau d'échange de matière (4) et le côté inférieur (26) du plateau d'échange de matière agencé directement au-dessus (4) se situe dans une plage allant de 0 à 0,3, notamment dans une plage allant de 0 à 0,2.
  8. Colonne (1) selon l'une quelconque des revendications précédentes, caractérisée en ce que la conduite de circulation (11) et l'ouverture de recyclage (14 ; 14-1 à 14-3) sont agencées de telle sorte que le liquide recyclé entre radialement dans la cavité de colonne (3).
  9. Colonne (1) selon l'une quelconque des revendications précédentes, caractérisée en ce que plusieurs ouvertures de recyclage espacées les unes des autres (14-1, 14-2, 14-3) sont formées dans le corps de colonne (2), et sont chacune en connexion fluidique avec la conduite de circulation (11).
  10. Colonne (1) selon l'une quelconque des revendications précédentes, caractérisée en ce que les bords supérieurs (23) du corps cylindrique (8) forment des bords de débordement, et le rapport entre l'écart vertical entre la zone la plus basse (L1) de la surface de collecte (5) du plateau d'échange de matière (4) et le bord inférieur (24) de l'ouverture d'évacuation (10) et l'écart vertical entre la zone la plus basse (L1) de la surface de collecte (5) du plateau d'échange de matière (4) et la hauteur (L5) du bord de débordement le plus inférieur du corps cylindrique (8) se situe dans une plage allant de 0 à 0,1, notamment dans une plage allant de 0 à 0,05.
  11. Colonne (1) selon l'une quelconque des revendications précédentes, caractérisée en ce que les ouvertures de recyclage (14-1, 14-2, 14-3) sont agencées par rapport aux corps cylindriques (8) de telle sorte qu'un écoulement de fluide en méandres (19) soit obtenu sur la surface de collecte (5) du plateau d'échange de matière (4).
  12. Colonne (1) selon l'une quelconque des revendications précédentes, caractérisée en ce que le plateau d'échange de matière (4) est un plateau à cheminées et le corps cylindrique (8) est un corps à cheminée.
  13. Procédé de séparation thermique entre au moins un gaz ascendant dans une colonne (1) selon l'une quelconque des revendications 1 à 12 et au moins un liquide descendant dans la colonne (1).
  14. Procédé selon la revendication 13, caractérisé en ce que du liquide est introduit par l'ouverture de recyclage (14 ; 14-1 à 14-3) en dessous du niveau du liquide (22) sur la surface de collecte (5).
  15. Procédé selon la revendication 13 ou 14, caractérisé en ce que le gaz ascendant et/ou le liquide descendant contiennent des monomères (méth)acryliques.
EP15747794.4A 2014-08-05 2015-08-04 Colonne et procédé de traitement thermique d'un fluide comprenant un conduit de retour Active EP3177379B1 (fr)

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US201462033157P 2014-08-05 2014-08-05
DE102014215437.5A DE102014215437A1 (de) 2014-08-05 2014-08-05 Kolonne zur thermischen Behandlung eines Fluids
PCT/EP2015/067943 WO2016020374A1 (fr) 2014-08-05 2015-08-04 Colonne de traitement thermique d'un fluide comprenant un conduit de retour

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CN110613856B (zh) * 2019-09-16 2021-04-16 宁波方太厨具有限公司 一种食具消毒柜

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CN106794387B (zh) 2019-11-29
EP3177379A1 (fr) 2017-06-14
US9958201B2 (en) 2018-05-01
DE102014215437A1 (de) 2015-11-05
CN106794387A (zh) 2017-05-31
US20160040929A1 (en) 2016-02-11
WO2016020374A1 (fr) 2016-02-11

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